Magnetic and Dielectric Losses of a Nanocomposites

Polymer Matrix Reinforced with Ferromagnetic

Powders

Vlad – Andrei Scarlatache, Marius Olariu, Stefan Massimo Pasquale

Ursache, Romeo Cristian Ciobanu Istituto Nazionale di Ricerca Metrologica
Department of Electrical Measurements and Materials Torino, Italy
The “Gheorghe Asachi” Technical University of Iasi m.pasquale@inrim.it
Iasi, Romania
vscarlatache@ee.tuiasi.ro

Abstract—This paper illustrates the effects of ferromagnetic
nanoparticles on dielectric and magnetic properties of a
polyolefinic adhesive polymer. The dielectric characteristics
analyzed were the real and imaginary part of complex
permittivity and dielectric losses of adhesive samples containing
iron oxide nanoparticles. The analyzed magnetic parameters
analyzed are the real and imaginary part of permeability and
magnetic losses. The measurements were performed in a
frequency range between 0.1 Hz to 10 MHz for dielectric
parameters and 1 MHz to 3 GHz in case of magnetic
permeability. Temperature was also varied between 30 ºC to 100
ºC, with 10 ºC increment.
Keywords – permeability; permittivity; dielectric and magnetic
losses;
I. INTRODUCTION
Joining of thermoplastics by electromagnetic implant
welding is a mature process. Presently, little information is
found in the literature to describe the relationship between the
properties of magnetic susceptor particles and the plastic
matrix materials into which they are dispersed, and their
interaction with high frequency electromagnetic fields [1].
Magnetic implant welding uses susceptors that couple, due
to ferromagnetic hysteresis, with high frequency
electromagnetic radiation to generate controllable heat in the
adhesive. Sometimes when the temperature increase, the
magnetic or dielectric resonance is shifting to different
frequency.
Melting temperature of this kind of thermoplastic adhesives
is around of 150 ºC, sow if this kind of material is supposed to
electromagnetic field it’s possible to melt for a given power
when inside of thermoplastic adhesive are inserted
ferromagnetic particles.
II. DESCRIPTION OF MATERIALS AND MEASUREMENT
SYSTEMS
The samples were prepared by inserting iron oxide
nanoparticles into a thermoplastic polyolefin polymer in order
to observe their dielectric and magnetic behavior as while
varying the frequency and temperature as well.
The production method of samples is based on a thermal
mixing on the teflon films, therefore major differences appear
in thickness, and for leveling a thermal press was used.
N type nanoparticles 4-6 nm
N 10%
20 N 20% C powder
N 30%
C type nanoparticles20-30nm
FMR freq (GHz)

C 10%
plastic. In this paper we analyze the effect of temperature on C 30%
magnetic and dielectric properties of a thermoplastic matrix
with insertion of susceptors based on iron oxide nanoparticles.
Npowder
Previously another study on this type of matrix was performed
at ambient temperature [2].
After performing the measurements it was concluded that
the small nanoparticles with diameter 4 ÷ 6 nm (Type N) have 0
a lower frequency of ferromagnetic response than nanoparticles 0 1000 2000 3000 4000
with diameter of 20 ÷ 30 nm (Type C). This behavior is Applied field (G)
illustrated in Fig. 1.
The possibility to analyses the magnetic and dielectric Figure 1. The FMR peak positions as a function of the applied magnetic
field for different MNPs powders (solid squares) and with MNPs dispersed in
losses will provide us an idea about the optimization of a Polyolefine matrix with different concentration. The solid lines are the linear
electromagnetic welding for this type of thermoplastic fit of the pure powder responses. frequencies [2].

EURODOC “Doctoral Scholarships for research performance at

European level”
 TABLE I APPLICABLE MATERIAL UNDER TEST (MUT) SIZE

Fixture Small Large

Holder A B C D
≥φ ≥φ ≥φ ≥φ
b 3.1 3.1 6 5
mm mm mm mm
≥φ ≥φ ≥φ ≥φ
c 8 6 20 20
mm mm mm mm
≥φ ≥φ ≥φ ≥φ
h 3 3 8.5 8.5
mm mm mm mm
Figure 3. The measurement system of magnetic characteristics at high
frequencies [4].

The results were analyzed with WinDeta software from

Novocontrol and saved in ASCII format. Diagrams and plots
were realized in Origin.

III. EXPERIMENTAL RESULTS

Figure 2. The measurement system of dielectric characteristics at low
frequencies [4].
For dielectric measurements the sample was prepared with
circle disk geometry of 20 mm in diameter. As describe in the
Table 1, for magnetic analysis is necessary to make more types
of ring samples with different diameters[3].
Two samples were prepared, one with inner diameter of 4
mm and outer of 6 mm, for small holders, and another one with
inner diameter of 7 mm and outer of 19 mm, for large holders.
The measurement system used to analyze the dielectric
properties in the frequency and temperature variation is
composed of an impedance analyzer Alpha - A from
Novocontrol, a ZGS cell and a temperature control system
Quatro Cryosistem, Fig. 2.
Alpha – A impedance analyzer have a band of frequency
from 0.001 Hz to 10 MHz, high phase accuracy (2.10-3 °) and
The frequency was varied between 0.1 Hz ÷ 106 Hz, with a
logarithmic scale and a number of 43 measurement points. The
temperature was increased from 30 ºC up to 100 ºC, with a step
of 10 ºC.
From Fig. 4, it is observed that while increasing
temperature, polar character of the samples is more
pronounced, exhibiting strong interfacial polarization while
increasing temperature, polarization which is specific for this
type of materials [5]. Dielectric constant decreases when the
frequency is increasing. Comparing the real and imaginary
permittivity one can observe a resonance phenomenon at
frequency around 10 kHz, which is attributed to the orientation
of nanoparticles in the field. This polarization is shifting
towards higher frequencies while increasing temperature, as it
can be observed from Fig. 5 and 6. Dielectric losses are
strongly influenced by temperature and frequency on these
materials.
Eps' 30 (°C)
Eps' 40 (°C)
Eps' 50 (°C)
5 Eps' 60 (°C)
Eps' 70 (°C)
Eps' 80 (°C)
Eps' 90 (°C)
Eps' 100 (°C)
Eps'

loss factor tan(δ) absolute accuracy (3.10-5) for low loss

dielectric materials and isolators broadband characterization.
Quatro Cryosystem have a range of temperature between -160
ºC to + 400 ºC, with a ramps from 0.01 °C / min to 20 °C / min
4
and a stability of 0.01 °C.
For magnetic measurements an impedance analyzer was
employed (Agilent E4991A with magnetic material test fixture
0.1 1 10 100 1000 10000 100000 1000000 1E7
Agilent 16454A), Fig.3. This system has a band of frequency
Frequency (Hz)
from 1 MHz to 3 GHz. For variation of temperature will use a
compressor CP5050N Black&Decker.
Figure 4. The real permittivity of thermoplastic adhesive samples with
insertion of 10% iron oxide particles type C.
 1.6
1
1.5
Eps" 30 (°C)
Eps" 40 (°C) 1.4
Eps" 50 (°C)
Eps" 60 (°C) 1.3
Eps" 70 (°C)
Eps" 80 (°C) 1.2
0.1
Eps" 90 (°C)
Eps"

Eps" 100 (°C)

u'
1.1

1
u' S-A
u' S-B
0.01 0.9 u' L-C
u' L-D
0.1 1 10 100 1000 10000 100000 1000000 1E7
0.8
Frequency (Hz) 1E7 1E8 1E9
Frequency [Hz]
Figure 5. The imaginary permittivity of thermoplastic adhesive samples with
insertion of 10% iron oxide particles type C.

1 u'' S-A
u'' S-B
u'' L-C
Tan(Delta) 30 (°C) u'' L-D
Tan(Delta) 40 (°C)
0.1
Tan(Delta) 50 (°C) 0.1
Tan(Delta) 60 (°C)
Tan(Delta) 70 (°C)
u"

Tan(Delta) 80 (°C)
Tan(Delta)

Tan(Delta) 90 (°C)
0.01
Tan(Delta) 100 (°C)

0.01
1E-3

1E7 1E8 1E9

0.1 1 10 100 1000 10000 100000 1000000 1E7 Frequency [Hz]
Frequency (Hz)

Figure 7. Real and imaginary permittivity of the sample N10% in the

Figure 6. The dielectric losses of thermoplastic adhesive samples with frequency range 1 MHz ÷ 3 GHz.
insertion of 10% iron oxide particles type C.
2
For studying the magnetic measurement accuracy of the
four types of holders was chosen to analyze the polymer u' 30 (°C)
sample with a volume of 10% nanoparticles N-type. As shown u' 40 (°C)
in Fig. 7 and as shown in the cell’s technical data sheet, type C u' 50 (°C)
u' 60 (°C)
and D holders have permeability values closely and linear.
u' 70 (°C)
Measuring scale is logarithmic with a total of 48 points in u' 80 (°C)
u' 90 (°C)
the frequency range from 1 MHz to 3 GHz.
u'

u' 100 (°C)

Nonlinear evolution of permeability values is primarily due
to low viscosity of material.
Analyzing the permeability for ambient temperature, one
can notice a slight decrease of values at frequencies lower than
100 MHz. Above this value a peak around the frequency of 500 1
MHz can be observed. 1E7 1E8
Frequency (Hz)
Analyzing the at imaginary permeability, which decreases
while increasing frequency up to 200 MHz. After this
frequency the imaginary permeability increasing substantially. Figure 8. Real permeability of the sample N10% in the frequency band 10
MHz ÷ 0.7 GHz to temperature variation from 30 to 100 °C.
Magnetic resonance can be noticed at a frequency around of
400MHz.
 Analyzing the imaginary permeability and magnetic losses
u" 30 (°C) in Fig. 9 and Fig. 10, a decrease of both parameters while
10 u" 40 (°C)
u" 50 (°C)
increasing frequency, can be noticed.
u" 60 (°C)
1 u" 70 (°C) IV. CONCLUSIONS
u" 80 (°C)
u" 90 (°C) For ring samples with higher diameter we have a good
0.1 u" 100 (°C) accuracy of measurements.
Sample C10% presents an orientational polarization at
u"

0.01
frequency around 10kHz and the sample N10% has a magnetic
resonance around the frequency of 300 MHz.
1E-3
With temperature increasing both dielectric and magnetic
losses increase.
1E-4

V. AKNOWLEDGMENT
1E7 1E8
Frequency (Hz) This paper was realized with the support of:
• EURODOC “Doctoral Scholarships for research
Figure 9. Imaginary permeability of the sample N10% in the frequency band
10 MHz ÷ 0.7 GHz to temperature variation from 30 to 100 °C.
performance at European level” project, financed by
the European Social Found and Romanian
Government;
0.1 • PERFORM-ERA “Postdoctoral Performance for
Integration in the European Research Area” (ID-
57649), financed by the European Social Fund and the
0.01
Romanian Government.
• POSDRU CUANTUMDOC “DOCTORAL
STUDIES FOR EUROPEAN PERFORMANCES IN
Tan(Delta)

1E-3 RESEARCH AND INOVATION” ID79407 project

Tan(Delta) 30 (°C)
Tan(Delta) 40 (°C)
Tan(Delta) 50 (°C)
Tan(Delta) 60 (°C)
1E-4
Tan(Delta) 70 (°C)
Tan(Delta) 80 (°C)
Tan(Delta) 90 (°C)
Tan(Delta) 100 (°C)
1E-5
1E7 1E8
Frequency (Hz)
Figure 10. Magnetic losses of the sample N10% in the frequency band 10
MHz ÷ 0.7 GHz to temperature variation from 30 to 100 °C.
Due to low accuracy of results which appears at the
beginning and the end of the frequency band, for temperature
variation was chosen frequency range 10 MHz ÷ 0.7 GHz.
In Fig. 8 it can be observed that the real part of
permeability, is strongly dependent on temperature, and
increasing with temperature. At low temperatures, permeability
does not have a high dependence of frequency when increasing
temperature but it has a downward trend with frequency. As for
the ambient temperature, around the frequency of 300 MHz we
have a peak and on the opposite side, on the descendent part of
this characteristic, a peak of the imaginary permeability can be
seen, peak characteristic to magnetic resonance. Practically, at
this frequency, the highest level of conversion from
electromagnetic energy in thermic energy is reached.
funded by the European Social Found and Romanian
Government;
Also a contribution for development of this paper, it have
the Polimag project as a source of the polymer samples:
• Regione Piemonte POR-FESR Asse I Innovazione e
transizione produttiva I.1.3 Innovazione e P.M.I.
• Partners POLIMAG: Coord MECT, CRF, INRIM,
VABER, KGR, UPO.
REFERENCES
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materials in high frequency magnetic fields,” Ashland Specialty
Chemical Co., 2006.
[2] A. Caprile, M. Coïsson, F. Fiorillo, P. Kabos, O. M. Manu, E. S.
Olivetti, M. A. Olariu, M. Pasquale, V. A. Scarlatache, “Microwave
behaviour of polymer bonded Iron oxide nanoparticles,” International
Magnetics Conference, INTERMAG, 2012.
[3] Agilent 16454A Magnetic Material Test Fixture, Operation and Service
Manual, Agilent Technologies, Part No. 16454-90020, 2008.
[4] http://tinyurl.com/9ewzrzf.
[5] V.A. Scarlatache, M. Ursan, R. C. Ciobanu, “Dielectric Properties
Characterization of Conductive Polymeric Materials at Temperature and
Frequency Variation,” OPTIM 2010 - 12th International Conference on
Optimization of Electrical and Electronic Equipment, Brasov, Romania,
May 20-22, 2010.